Sodium Carbonate → {8-Fluoro-1,4-dioxaspiro[4.5]decan-8-yl}methanol

HRID 1043233ノート

反応式

HRID 1043233 の反応式
[FH:1].N1C=CC=CC=1.O1[C:10]2([CH2:19][CH2:18][CH2:17][CH2:16][C:13]3([O:15][CH2:14]3)[O:12][CH2:11]2)C1.[C:20]([O-:23])([O-])=O.[Na+].[Na+]>ClCCl>[F:1][C:18]1([CH2:20][OH:23])[CH2:17][CH2:16][C:13]2([O:12][CH2:11][CH2:14][O:15]2)[CH2:10][CH2:19]1

参加物

6

反応物 4

HCID 10340Sodium CarbonateHCID 64774Pyridine, hydrofluoride (1:1)HCID 86647914HCID 86647914、化合物HCID 178435160HCID 178435160、化合物

生成物 1

HCID 67225989{8-Fluoro-1,4-dioxaspiro[4.5]decan-8-yl}methanol

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

A solution of pyridine hydrofluoride (4 g) in dichloromethane (10 mL) was added dropwise to a solution of EXAMPLE 443A (1.7 g) in dichloromethane (20 mL) in a polyethylene bottle at 0° C. The mixture was stirred at room temperature overnight. The mixture was carefully poured over a mixture of ice-water and Na2CO3 and extracted with ethyl acetate (2×300 mL). After washing with water and brine, the organic layer was dried over Na2SO4, and filtered. Concentration of the filtrate gave the crude product.

後処理

  1. extractionextracted with ethyl acetate (2×300 mL)
  2. washAfter washing with water and brine
  3. dry with materialthe organic layer was dried over Na2SO4
  4. filtrationfiltered

出典と根拠

ORDレコード
ord-816022b831694ddcb7d88497577ac72f
出典データセット
uspto-grants-2013_10
特許番号
US08557983B2

反応ノート

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